Water → Methyl 3-chloro-p-anisate

HRID 1283640

반응식

HRID 1283640 반응식
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([Cl:11])[CH:5]=1.[OH-].[Na+].O.S(OC)(O[CH3:20])(=O)=O>CCOCC>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:20])=[C:6]([Cl:11])[CH:5]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 77580Methyl 3-chloro-4-hydroxybenzoate

생성물 1

HCID 123469Methyl 3-chloro-p-anisate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a cooled solution of 14.5 g. (0.078 mol.) of 3-chloro-4-hydroxybenzoic acid methyl ester and 4.0 g. (0.1 mol.) of sodium hydroxide in 100 ml. of water was dropwise added 9.8 g. (7.3 ml., 0.079 mol.) of dimethyl sulfate. The reaction mixture was refluxed for two hours. After cooling, ether was added and the layers were separated. The organic phase was washed with water, dilute sulfuric acid and water, dried (Na2SO4) and concentrated in vacuo to give 3-chloro-4-methoxybenzoic acid methyl ester, m.p. 72°-74°.

후처리

  1. temperatureThe reaction mixture was refluxed for two hours
  2. temperatureAfter cooling
  3. customthe layers were separated
  4. washThe organic phase was washed with water, dilute sulfuric acid and water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e844daecefa24991bf40461d7faffdea
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03975537

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